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Methanol → Methyl 3-bromo-2,6-dimethoxybenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 3-Bromo-2,6-dimethoxybenzoic acid | HCID 2774744 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl 3-bromo-2,6-dimethoxybenzoate | HCID 21886016 | 78.9% |
反応手順
3-Bromo-2,6-dimethoxybenzoic acid (5.0 g, 19.2 mmol) and thionyl chloride (10 ml) were heated to reflux for 2 h. The mixture was then concentrated in vacuo and diluted with CH2Cl2 (20 ml) and added to a solution of MeOH (614 mg, 38.4 mmol) and triethylamine (3.88 g, 38.4 mmol) in CH2Cl2 (100 ml) at 0° C. The resulting mixture was allowed to warm to RT and stirred for 64 h. The organics were washed with 10% HCl (50 ml), brine (50 ml) and dried (MgSO4) and purified by chromatography (0–50% EtOAC in heptane) to leave a white solid (4.17 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07138527B2 |
| 出典データセット | uspto-grants-2006_11 |
| ORD ID | ord-6457be78d84249448fa0ee2b08f904df |
| 出典メモ | uspto-grants-2006_11 |